Transcript
Operating Instructions
Version 4.x
Refractometers
RE40D/RE50
Contents
Contents
Page
1.
Introduction ...................................................................................................................... 7
2.
Safety measures ............................................................................................................... 9
3. 3.1 3.2 3.3
Refractive index .............................................................................................................. 10 Definition of the refractive index ......................................................................................... 10 Measuring principle .......................................................................................................... 11 Anatomy of the measuring cell ........................................................................................... 11
4. 4.1 4.2 4.3
The instrument ................................................................................................................ 12 Front and rear view .......................................................................................................... 12 Keypad ........................................................................................................................... 14 Display ........................................................................................................................... 17
5.
Measures for correct measurements ................................................................................ 18
6. 6.1 6.1.1 6.1.2 6.2 6.2.1 6.2.2 6.2.3 6.2.4 6.2.5 6.2.6 6.3 6.4 6.4.1 6.4.2
Getting started ................................................................................................................ 20 Setting up the measuring system ....................................................................................... 20 Connecting an SC1 or SC30 automation unit ....................................................................... 20 Connecting the printer and the barcode reader ..................................................................... 20 Setting up the RE Refractometer ......................................................................................... 21 Setting up the peripheral instruments .................................................................................. 21 User and country specific settings ...................................................................................... 23 Activating the automatic error detection ............................................................................... 23 Setting up the instrument test ............................................................................................. 24 Entering the method for adjustment .................................................................................... 24 Entering the method for measurements ............................................................................... 26 Adjusting the RE Refractometer .......................................................................................... 28 Performing an instrument test and measurements ................................................................ 30 Performing instrument test and measurement manually or with SC1 ...................................... 30 Performing instrument test and measurements with SC30 ..................................................... 32
7. 7.1 7.2 7.2.1 7.2.2
Sample (number/identification) and sample file ............................................................... 35 Menu to enter data for a single sample ............................................................................... 35 Menu to enter a sample file (sample changer) ..................................................................... 36 Creating a sample file using a dialogue format (Create) ....................................................... 37 Creating a sample file using a table format (Edit) ................................................................ 39
8.
Report (password protected) ........................................................................................... 40
9. 9.1 9.2 9.3 9.4 9.5
Measuring parameters (password protected) .................................................................... 41 Method Name .................................................................................................................. 42 Measuring temperature (Meas.Temp.) ................................................................................ 42 Measurement stability (Stability) ........................................................................................ 42 Waiting time (Wait Time) .................................................................................................. 43 Sequence (Sequence: sampling, draining, rinsing, purging) ................................................. 43
METTLER TOLEDO RE40D/RE50 Refractometers
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Contents
Contents
Page
10. 10.1 10.1.1 10.2 10.2.1 10.2.2 10.3
Calculation parameters (password protected) .................................................................. 46 Result (refractive index, Brix, HFCS, concentration) .............................................................. 46 Calculating concentrations, converting into other units (Conc.) .............................................. 48 Temperature compensation ............................................................................................... 51 Entering a temperature compensation table ......................................................................... 52 Input of a coefficient for temperature compensation .............................................................. 53 Decimals ........................................................................................................................ 54
11. 11.1 11.1.1 11.1.2 11.1.3 11.2 11.3 11.4 11.5 11.6 11.7 11.7.1 11.7.2 11.8 11.8.1 11.8.2 11.8.3 11.9 11.10
Functions (password protected) ....................................................................................... 55 Stored results (Function 0: Data File) ................................................................................. 55 Statistical evaluations ....................................................................................................... 56 Recalculations ................................................................................................................. 57 Marking stored results as invalid ........................................................................................ 58 Sample file (Function 1: Sample File) ................................................................................. 58 Method file (Function 2: Method File, RE50 only) ................................................................ 59 Automation units (Function 3 {2}: Changer) ....................................................................... 59 Connecting a DE Density Meter (Function 4 {3}: DE Connect) ............................................... 61 Configuring the instrument test (Function 5 {4}: Set Check) .................................................. 61 Periodic instrument tests and adjustments (Function 6 {5}: Periodic) .................................... 63 Periodic instrument tests ................................................................................................... 63 Periodic adjustments ........................................................................................................ 64 Multiple measurements (Function 7 {6}: Multiple Meas.) ...................................................... 66 Starting measurements automatically (Auto Start) ................................................................ 67 Automatic statistical evaluations (Auto Statistics) ................................................................. 67 Automatic error detection (Repeat Meas.) ............................................................................ 69 Memory card functions (Function 8: Card Utility, RE50 only) ................................................. 70 Clearing the memory (Function 9 {7}: Memory Clear) .......................................................... 71
12. 12.1 12.1.1 12.1.2 12.1.3 12.2 12.3 12.3.1 12.3.2 12.4 12.5 12.6
Setup (password protected) ............................................................................................. 72 Interfaces (Setup 0: Interface) ............................................................................................ 72 Setting up the RS-232C interface for the computer (RS-232C) ............................................... 72 Setting up the interface for the printer (Printer) ..................................................................... 73 Setting up the interface for the barcode reader (Barcode(AUX)) .............................................. 73 Date and Time (Setup 1: Date & Time) ............................................................................... 74 Operator names / Units (Setup 2: Op.Names/Units) ............................................................. 75 Concentration Units .......................................................................................................... 75 Operator Names ............................................................................................................... 76 Serial/Version number (Setup 3: Serial/Version) ................................................................... 76 LCD contrast (Setup 4: LCD Contrast) ................................................................................. 77 International (Setup 5: International) .................................................................................. 77
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METTLER TOLEDO RE40D/RE50 Refractometers
Contents
Contents
Page
12.7 12.8 12.9 12.10
Password lock (Setup 6: Lock) .......................................................................................... 77 Beep (Setup 7: Beep) ....................................................................................................... 78 Temperature adjustment (Setup 8: Temp.Adjust) .................................................................. 78 Type of adjustment (Setup 9: Calibration Mode, RE50 only) .................................................. 79
13. 13.1 13.1.1 13.1.2 13.1.3 13.1.4 13.1.5 13.1.6 13.1.7 13.1.8 13.1.9 13.1.10 13.1.11 13.1.12 13.1.13 13.2 13.2.1 13.2.2 13.2.3 13.2.4
Memory Cards (RE50 only) ............................................................................................. 82 Data memory cards .......................................................................................................... 82 Displaying the available and used storage space ................................................................. 82 Saving results .................................................................................................................. 83 Deleting results ................................................................................................................ 83 Loading results ................................................................................................................ 84 Saving methods ............................................................................................................... 85 Deleting methods ............................................................................................................. 86 Loading methods ............................................................................................................. 86 Saving sample files .......................................................................................................... 87 Deleting sample files ........................................................................................................ 87 Loading sample files ........................................................................................................ 88 Saving instrument tests and adjustment data ....................................................................... 88 Deleting instrument test and adjustment data ...................................................................... 89 Loading instrument tests and adjustment data ..................................................................... 89 Memory cards for special applications ................................................................................ 90 Loading tables into the instrument (Install table) .................................................................. 90 Using concentration tables in methods ............................................................................... 91 Using temperature compensation tables in methods ............................................................. 91 Loading tables back onto the memory card (Uninstall Table) ................................................ 92
14. 14.1 14.2
Error messages and malfunctions .................................................................................... 93 Error messages ................................................................................................................ 93 Malfunctions .................................................................................................................... 94
15. 15.1 15.2 15.3
Maintenance ................................................................................................................... 95 Cleaning the measuring cell .............................................................................................. 95 Internal battery ................................................................................................................. 95 Main power supply voltage, mains fuse .............................................................................. 95
16. 16.1 16.2
Standard and optional equipment .................................................................................... 96 Standard equipment ......................................................................................................... 96 Optional equipment .......................................................................................................... 96
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Contents
Contents
Page
Appendix1: Refractive index table for pure water ............................................................................. 100 Appendix2: BRIX table .................................................................................................................... 101 Appendix3: HFCS42 and HFCS55 (inverted sugars) .......................................................................... 102 A.3.1 HFCS42 table (0 to 76 solids%) ..................................................................................... 103 A.3.2 HFCS55 table (0 to 80 % solids) .................................................................................... 104 Appendix4: A.4.1 A.4.2 A.4.3
Barcode reader ............................................................................................................. 105 Configuration of the METTLER TOLEDO DLC7070 barcode reader ........................................ 105 Special characters .......................................................................................................... 105 Operator names ............................................................................................................. 106
Technical data RE40D Refractometer ................................................................................................ 107 Technical data RE50 Refractometer .................................................................................................. 108
Index ................................................................................................................................ 109
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METTLER TOLEDO RE40D/RE50 Refractometers
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METTLER TOLEDO RE40D/RE50 Refractometers
Introduction
1.
Introduction
The RE40D and RE50 Refractometers are used for the simple determination of the refractive index of liquid samples. The measurements are done using a method based on total reflection. With this method even dark samples may be measured without any difficulty. The RE Refractometers are practically maintenance-free, thanks to the latest technical developments – no moving parts, long-life LED light source and inert sapphire prism. The RE40D and RE50 Refractometers – measure samples with a refractive index in the range of 1.3200 … 1.7000 (RE40D) or 1.32000 … 1.58000 (RE50). – need a minimum amount of sample (approximately 0.4 milliliters) for measurement. – keep the temperature of the sample being measured constant in the range of 15.0 to 70.0°C (RE40D) or 15.00 to 50.00°C (RE50) by means of a built-in Peltier thermostat (no water bath necessary). – calculate the samples' refractive indices for any reference temperature based on user-defined temperature functions. – display the refractive index of the samples directly in Brix degrees or in HFCS (High Fructose Corn Syrup, RE50 only) if so desired. – are capable of directly converting and displaying the measurement values into any other units (e.g. Zeiss) based on user-defined formulas. – are suitable for determination of concentrations. Concentrations are automatically calculated based on the refractive indices according to user-defined formulas or concentration tables. – provide statistical evaluations (mean, standard deviation, relative standard deviation) of the results. – allow entry of ten measuring methods. One of these methods is reserved for adjustment (calibration) of the instrument. – can be tested easily with the built-in check function. This function allows regular testing of the accuracy of measurement without changing the instrument's settings. – have three serial interfaces to connect a printer, a barcode reader and a computer, as well as a port to control an automation unit (SC1 or SC30, see following page). The RE50 Refractometer – stores methods, measured data and sample files on memory cards. As a result, transferring methods to another RE50 Refractometer poses no problem at all.
METTLER TOLEDO RE40D/RE50 Refractometers
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Introduction
Important: An SC1 or an SC30 Sample Delivery and Cleaning Unit (option) turn your RE Refractometer into a fully automated measuring system for the measurement of individual samples (SC1) or series of samples (SC30). The Sample Delivery and Cleaning Units not only reduce the work involved in the determination of refractive index, they also help to prevent measurement errors, save cleaning solutions and increase safety in the workplace. The procedure for doing measurements, adjustments and tests of the measurement accuracy of the RE Refractometer depends on whether the instrument is operated manually or together with an automation unit (SC1 or SC30). For this reason, the paragraphs are marked in these Operating Instructions as follows: These paragraphs you have to observe only if you operate your RE Refractometer manually (i.e. without SC1 or SC30 automation unit).
These paragraphs you have to observe if you operate your RE Refractometer with an SC1 Sample Delivery and Cleaning Unit for the measurement of individual samples.
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These paragraphs you have to observe if you operate your RE Refractometer with an SC30 Sample Delivery and Cleaning Unit for the measurement of sample series (sample changer).
METTLER TOLEDO RE40D/RE50 Refractometers
Safety measures
2.
Safety measures
The RE40D and RE50 Refractometers have been tested for the intended purposes documented in these Operating Instructions. However, this does not absolve you from the responsibility of performing your own tests wether the product supplied by us is suitable for your intended methods and purposes. You should, therefore, observe the following safety measures. Measures for your protection – Ensure that you plug the power cable supplied into a socket which is grounded! A technical defect could be lethal in the absence of grounding. – Switch the instrument off and disconnect the power cable when you change blown fuses! An electric shock could be lethal. – Do not use the instrument in areas with danger of explosion! The housing of the RE Refractometers is not gas tight (danger of explosion due to spark formation, corrosion by gas seeping into the instrument).
Measures for operational safety – Clean the prism immediately after a measurement of strong acids and bases. They can damage the prism or the stainless steel cone. – Only use fuses of the specified type when they need to be exchanged. – Exclude the following environmental influences: • powerful vibrations • direct sunlight and sudden changes in temperature • corrosive gases • very dusty environment • high atmospheric humidity • temperatures below 5 °C and above 35 °C • strong drafts • powerful electric or magnetic fields which influence the power supply trough large load fluctuations. – To apply the samples do not use any hard objects such as metal, glass or ceramic as they could damage the prism. – If the instrument is not going to be used for a longer period of time, clean the prism before putting the instrument away. We recommend storing the instrument in the cardboard box in which it was delivered. – Avoid storage under excessive ambient conditions such as too high or too low temperatures; high humidity or very dusty areas will damage the instrument.
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Refractive index
3.
Refractive index
3.1
Definition of the refractive index
The refractive index n of a substance is the ratio of the velocity of a ray of light in a vacuum to its velocity in the medium (unitless).
n1 e.g. Air
If a ray of light passes from an optically less dense medium to a denser one (e.g., from air to water) at a particular angle, it changes direction; if the incident light meets the new medium vertically, there is no change in direction. According to Snell's law of refraction, the ratio of the refractive indices of the two media is proportional to the ratio of the angle of refraction and the angle of incidence of the ray of light:
n2 e.g. Water
n1 sin β = n2 sin α
If a ray of light passes into an optically less dense medium from a denser one, it also changes direction. If the angle of incidence α is increased, it reaches a critical value at which the ray of light no longer passes into the less dense medium (angle of refraction β = 90°). When exceeding this "critical angle", total reflection occurs. The critical angle α is used to calculate the refractive index:
Air
Water
Critical angle
Total reflexion
β = 90°
sin β = 1
As the refraction depends on the wavelength of the incident light, the standard refractive index n is measured at the D line of sodium (wave length 589.3 nm) and symbolized by nD. The refractive index depends not only on the wavelength of the incident light, but also on the temperature of the sample being measured. The standard temperature is 20 °C. If measurements are performed at a different temperature, e.g., 25 °C, this must be specified: n25 . D
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METTLER TOLEDO RE40D/RE50 Refractometers
Refractive index
3.2
Measuring principle The light emitted by light source passes through the prism and encounters the sample. It is partially refracted (angle of incidence < critical angle) and partially reflected (angle of incidence > critical angle).
Sample
Prism
The reflected light is recorded using an optical sensor (CCD). The boundary between the dark and light areas represents the critical angle needed to calculate the refractive index.
Light source Optical sensor (CCD)
3.3
Anatomy of the measuring cell
The light source is a light emitting diode (LED) whose beam passes through a polarizing filter, an interference filter (589.3 nm) and various lenses before it passes through the sapphire prism and hits the sample. The reflected light (angle of incidence > critical angle) is led via a lens to the optical sensor, which records the critical angle. The temperature at the intermediate prism/sample zone is measured by a built-in sensor.
Lens Lens Interference filter
Prism Lens Measuring cell
Polarizing filter
Light source
METTLER TOLEDO RE40D/RE50 Refractometers
Optical sensor (CCD)
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The instrument
4.
The instrument
4.1
Front and rear view
Front view 4. Cover lid 5. Thread for flow cell 6. Measuring cell
7. Prism 1. LC display
2. Keypad
3. Memory card slot
Rear view
8. Printer interface
9. AUX. interface (barcode reader) 10. RS232C interface (computer) 13. Connector for automationunit (SC1, SC30)
11. Power switch
12. AC power connector 14. Connector for external pump
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METTLER TOLEDO RE40D/RE50 Refractometers
The instrument
General overview 1.
LC display Seven-line LCD to show the measurement results, conditions and settings.
2.
Keypad (alphanumeric) To start measurements, enter measurement conditions, calculation parameters, etc.
3.
Memory card slot To upgrade the instrument's software. To load and download data, methods and sample files (RE50 only).
4.
Cover lid When closed it protects the measuring cell and eliminates incoming light during measurement. When opened it prevents sample liquid from splashing to the rear of the instrument.
5.
Thread for flow cell (FCU) Thread to mount a flow cell unit (to connect an SC1 or SC30 automation unit).
6.
Measuring cell When doing measurements manually, the sample is pipetted in the center of the stainless steel cone. The minimum amount of sample (0.4 mL) is indicated by a ring mark.
7.
Prism The prism is made of sapphire, which is strongly resistant to corrosion, very rigid and of high thermal conductivity.
8.
Interface for a printer To connect a serial matrix printer.
9.
Interface for a barcode reader (AUX.) To connect a barcode reader.
10. Interface for a computer (RS232C) To connect a computer (e.g. for data acquisition with the DataCapture software) or a METTLER TOLEDO DE40/45/51 Density Meter. 11. Power switch 12. AC power connector Connector for the mains cable. The RE Refractometers adapt automatically to the line voltage of a country as long as it is within the range of 100 to 240 V. 13. Connector for an automation unit (EXT.) Control connector for a Sample Delivery and Cleaning Unit (SC1 or SC30). 14. Connector for an external pump (EXT PUMP) For the automatic execution of sample measurements (e.g. of an reaction mixture in a reactor) in fixed time intervals a peristaltic pump may be connected here.
METTLER TOLEDO RE40D/RE50 Refractometers
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The instrument
4.2
Keypad
Display
Sample
Print
Report
Func.
Meas. Para
Setup
Calc. Para
7
8
9
ABC
DEF
GHI
4
5
6
JKL
MNO
PQR
1
2
3
STU
VWX
YZ
0
-
.
BLK
Check Calib.
BS
Rinse/ Purge Pump
Method
Enter Clear Escape
Reset
Measure
Sample
Sample
Entry of sample parameters such as sample number and ID. Entry of a sample file (with SC30).
Report
Report
Definition of the printing format for the results. Three formats are available: (1) Short: minimal printing format. (2) GLP: format complying with GLP requirements. (3) Variable: User defined format.
Meas. Para
Measuring Parameters
Definition of the measuring parameters: - Method name (8 characters, alphanumeric). - Stability (criteria for the acceptance of measurements). - Waiting time (prior to measurement, 0 … 9999 s). - Sample sequence used if the instrument is connected to an automation unit SC1 or SC30 (definition of the times for sampling, draining, rinsing and drying of the measuring cell).
Calc. Para
Calculation Parameters
Definition of the calculation parameters: - Selection of the unit for the result (nD, Brix, HFCS, concentration, etc.). - Selection of the calculation formula or entry of concentration tables for converting the measured refractive index into any other units. - Decimals for the results (refractive index, Brix, HFCS and calculated results). - Temperature compensation. Input of a formula or a table to covert the measured refractive indices to a temperature other than the measuring temperature.
The printing format as well as the measuring and calculation parameters ("Report", "Meas.Para" and "Calc.Para" keys) may be defined for each of the 9 measuring methods individually. 14
METTLER TOLEDO RE40D/RE50 Refractometers
The instrument
Method
Method
Select the measuring method (0 … 9). The method is selected by pressing the "Up", "Down" or the corresponding number key. Method 0 ("CALIB") is reserved for adjustment of the instrument.
Display
Display
Toggle between numerics, capital and small letters when entering text. Select result display (toggle between nD, Brix, HFCS and user defined units) after a measurement.
Print
Print measuring methods, stored results and instrument settings.
Function
Access to the following functions:
Print
Func.
40D (0) (1) (-)
50 (0) Data File: (1) Sample File: (2) Method File:
(2) (3) (3) (4) (4) (5)
(5) (6)
(6) (7)
(-) (8) (7) (9) Setup
Setup
Model ("(-)" = menu not available) Access to stored results. Enable/disable sample sequences (for SC30). Transfer methods from the instrument to a memory card and vice versa. Changer: Selection of the automation unit (SC1 or SC30). DE Connect: To connect a DE Density Meter. Set Check: Entry of the names and the nominal refractive indices of the standards used for daily and periodic instrument tests. Definition of the maximum deviation of the measured value accepted when doing instrument tests. Periodic: Definition of the intervals for periodic adjustments and instrument tests. Display of the stored adjustment and instrument test results. Multiple Meas.: Conduct multiple measurements of one sample. Enable/disable automatic error detection (only available with SC1 and SC30). Automatic statistics. CARD Utility: Handling of stored data on memory cards (e.g., load special applications). Memory Clear: Delete data stored in the instrument's memory.
Access to the following instrument settings: 40D 50 (0) (0) Interface:
Model ("(-)" = menu not available) Configure the serial interfaces (for printer, barcode reader and PC). (1) (1) Date&Time: Set date and time. (2) (2) Op.Names/Units: Entry of operator names and concentration units. (3) (3) Serial/Version: Display of the serial and version number of the instrument. (4) (4) LCD Contrast: Set contrast for the LC display. (5) (5) International: Select format for date and temperature (°C / °F). (6) (6) Lock: Limit access to certain functions with a password. Enable/disable and selection of type of acoustic signal. (7) (7) Beep: (8) (8) Temp.Calib: Execute adjustment of temperature measurement. (-) (9) Calibration Mode: Define type of adjustment. Check
Check
Perform an instrument test: daily (always active) or periodic (only when due).
METTLER TOLEDO RE40D/RE50 Refractometers
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The instrument
Calib.
Calibration
Perform an adjustment.
BS
Backspace
Backspace to delete characters.
Rinse/ Purge
Rinse/Purge
Only available if an automation unit (SC1, SC30) is connected to the instrument: Activates an automatic rinsing and purging cycle according to the settings in the sequence of method "0.CALIB".
Pump
Pump
Switch an external pump (connected to EXT PUMP) on/off.
Clear
Clear
Clear an entire input field or go back to the last setting (undo).
Esc.
Escape
Return to the main display (result of the last measurement is not deleted).
Reset
Reset
Abort a measurement and return to the main display (the result of the last measurement is deleted).
Measure
Start a measurement (or a measurement series, SC30).
0…9
Select an item from a list (menu, list with results, etc.) or enter an alphanumeric character (select capital/small letters or numerals with the
key). Press twice for B and three times for C. Enter a blank space with the <0 (BLK)> key.
Measure
7 ABC
.
Dot
–
Hyphen
When entering concentration units (menu "Setup/2.OP.Names/Units"): For "%" and "/" press the hyphen key twice or three times, respectively.
Enter
Confirmation of an entry. This key is referred to with in these Operating Instructions.
Enter
up left/right
Keys to move the cursor. The and keys are also used for selections in the menus. To select an option in a menu (Function/Setup). To select a method, results, etc. in a list. In the latter case, direct entry of the corresponding number via the alphanumeric keypad is usually quicker than using the arrow keys.
down
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METTLER TOLEDO RE40D/RE50 Refractometers
The instrument
4.3
Display
The RE Refractometers come equipped with a seven line LC display with 40 characters per line. When the instrument is switched on (rear of the instrument), the following message appears on the display: The software version ("Version") appears for a short time. The software version can also be displayed under "Setup/3.Serial/Version".
Refractometer
REXX 1 After a few seconds the main display appears. The message "Wait for Ready" blinks until the measuring cell has reached the set temperature. Then, if the measuring cell has been adjusted, the message "Ready" appears, if not, the message "No Calibration" appears.
1.Method-1 Temp.(° C) Set 20.00 Cell 20.00
Version X.XX
3
2
4
F 01-01 nD (None)
Out Wait for Ready
5 6 7
8
9
1.33299
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The following information is shown on the main display: 1 2 3
Number and name of the measuring method. Sample identification. This field can be empty (e.g., when the instrument is switched on for the first time). "F" appears when the sample file is turned on. This is always the case if an SC30 Sample Delivery and Cleaning Unit is attached. 4 Sample number. The sample number consists of two parts, e.g., 01- 02. The first two-digit number (ranging from 00 to 98) is the number of the measurement series. It is also referred to as the "High Sample No.". If you use your own specific series number for each type of sample when measuring various types of samples, it is easy to evaluate the stored results statistically afterwards. The next two digit number (ranging from 00 to 99) is the sample's number. In the instrument it is also referred to as the "Low Sample No.". This number is automatically increased by 1 after each measurement. 5 Status line. Status, error messages and instructions for the operator are displayed here. 6 Measured temperature of the refractive index measuring cell. 7 Set temperature of the measuring cell according to the currently selected measuring method. 8 Error message of the automatic error detection (only available if the RE Refractometer is used together with an SC1 or an SC30 Sample Delivery and Cleaning Unit). 9 Unit for the measured value according to the currently selected measuring method (nD, Brix(%), HFCS42, HFCS55, Conc.). 10 Measured value. The measured value only appears after having started a measurement. After completion of a measurement, the unit for the measured value may be selected with the key (e.g., nD or Brix(%)).
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Measures for correct measurements
5.
Measures for correct measurements
The RE Refractometer's "Repeat Meas." (automatic error detection, only available with attached SC1 or SC30 automation unit) and "Check" functions ensure that you can easily identify errors due to the instrument or the measured samples. To ensure correct measurements please pay attention to the following: – After turning on the instrument or changing the measuring temperature, it takes approximately 15 minutes for the measuring cell to reach the set temperature. To ensure correct measurements, however, you should give the instrument at least 30 minutes to stabilize the temperature of the measuring cell before you perform a measurement or an adjustment. – Adjust the instrument after each change of measuring temperature. – Check the measuring accuracy of the instrument regularly with refractive index standards. In section 16.2 you can find refractive index standards suitable for this purpose. – Ensure that the samples to be measured are homogeneous. Viscous and highly concentrated liquids must be mixed thoroughly before a sample is taken. – Use soft paper tissues or washed gauze to clean the measuring cell and to dry the prism. Never use cotton swabs for this purpose, as their fibers could adhere to the prism and cause faulty measurements. – Use deionized water to clean the cell after measuring aqueous samples. For organic samples use a suitable organic solvent such as toluene, ethanol or acetone. In order to speed up drying of the measuring cell, we recommend you use a second highly volatile solvent such as acetone to wipe the first one off. – Make sure that the ring mark is always covered by the sample when doing measurements (minimum sample volume: approximately 0.4 mL). – Prior to measurement always stir the sample on the prism carefully to allow air bubbles to escape.
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– For the first rinsing liquid ("RINSE 1") use a solvent capable of dissolving your samples. If you have to measure both aqueous samples and samples which contain oil and fat, you may use an aqueous solution with a surfactant as first rinsing liquid. Add approximately 25% v/v of ethanol to this surfactant solution in order to prevent excessive foam formation (during rinsing, the liquid is mixed with air!). – Use a highly volatile solvent (e.g., acetone) as second rinsing liquid in order to ensure a complete drying of the measuring cell. – Dismantle the flow cell (FCU) at certain time intervals and clean the surface of the prism with a soft paper tissue dampened with an appropriate cleaning solvent. After cleaning refit the flow cell unit and press the "Rinse/Purge" key on the Refractometer.
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METTLER TOLEDO RE40D/RE50 Refractometers
Measures for correct measurements
Take special care if the samples to be measured have properties such as described below: – Highly concentrated samples The concentration of such samples may change during the measurement due to evaporation of solvent. This may result in poor repeatability of results or a wide difference between the measured and the true value. When working at elevated temperatures, these errors are more likely to occur. If you must measure such samples: – if possible use an automation unit (SC1 or SC30). When working with a flow cell unit, an evaporation of the solvent during the measurements may be ruled out. Store the samples in METTLER TOLEDOS's sealable sample vials until they are measured. – do not perform the measurements at low temperatures, because this could lead to crystallization and thus to light scattering. – Colloidal samples (such as milk, etc.) Colloidal particles scatter light, which causes poor repeatability of the measured value. In the worst case, no measurement is possible.
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– Activate the "Repeat.Meas" function and enter a value of at least 3 for "Repetitions" (see section 11.8.3). Multiple measurements of each sample will then be performed and the mean value of the measurements is calculated and displayed. If the measurements are excessively affected by scattered light the message "Out" appears on the display and an error message is printed out.
– Highly volatile samples The measurements may take long or the results might be erroneous for the following reason: Part of the sample evaporates during the measurement and the surface of the prism is cooled down due to the evaporation energy. This may cause the temperature control of the measuring cell to malfunction. Therefore, when measuring such samples, set the measuring temperature as low as possible and cover the measuring cell with a vapor proof lid (ME 51322114), or use an automation unit (SC1 or SC30) for the measurements. Store the samples in METTLER TOLEDOS's sealable sample vials until they are measured. i
– Samples which tend to foam Foam or air bubbles on the surface of the prism scatter the light and cause poor repeatability of the results. In the worst case, no measurement is possible.
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Getting started
6.
Getting started
This section explains how to set up the RE Refractometer, adjust it and perform the first measurements. A practical example, the determination of the sugar content (BRIX) of orange juice, will familiarize you with the most important features of the RE Refractometer. We presume that you operate your RE Refractometer with a GA42 printer and a DLC7070 barcode reader. If this is not the case, you may skip the corresponding sections. Certain procedures to do the set up, measurements, adjustments and tests of measurement accuracy of the RE Refractometer and entering methods are different depending on whether you operate your measuring instrument manually or with an automation unit (SC1 or SC30). This section describes all the three possibilities, and the corresponding paragraphs are marked accordingly (see section 1).
6.1
Setting up the measuring system
6.1.1
Connecting an SC1 or SC30 automation unit Connect the SC1 or SC30 Sample Delivery and Cleaning Unit to your RE Refractometer as described in the Operating Instructions of the automation unit.
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6.1.2
Connecting the printer and the barcode reader
Connect the GA42 printer to the printer port of the RE Refractometer. Make sure that the DIP switch 2 on the printer is set to ON. The DIP switch can be found under the battery cover (see GA42 Operating Instructions). Connect the GA42 printer to the power supply. Connect the DLC7070 barcode reader to the "AUX." port of the RE Refractometer. Switch on the GA42 printer and the RE Refractometer (and the automation unit, if connected).
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METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
6.2
Setting up the RE Refractometer
6.2.1
Setting up the peripheral instruments
6.2.1.1 Automation unit
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Press the key on the RE Refractometer. Select "3.Changer" (or "2.Changer", RE40D) with the <3> (<2>) key and confirm with .
Select "SC1" for "Changer" with the key and confirm with . More options appear in the "Changer" menu: Select "On" for "Rinse / Purge" and for "Drain+Prerinse" with the key. Confirm both settings with .
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Select "SC30" for "Changer" with the key and confirm with . More options appear in the "Changer" menu: Select "Off" for "Calib.", "Home" for "Start Position" and "On" for "Rinse /Purge" and for "Drain+Prerinse" with the or key. Confirm all settings with .
< Function > 0.Data File 1.Sample File 2.Method File 3.Changer 4.DE Connect
5.Set Check 6.Periodic 7.Multiple Meas. 8.Card Utility 9.Memory Clear
< Changer > Changer Rinse / Purge Drain+Prerinse Exit
: :Off On :Off On :[Execute]
< Changer > Changer Calib. Start Position Rinse / Purge Drain+Prerinse
: :Off On :Home Current :Off On :Off On
An exact description of this menu can be found in section 11.4.
6.2.1.2 GA42 printer Press the key. Select "0.Interface" with the <0> key and confirm with .
< Setup > 0.Interface 1.Date & Time 2.Op.Names/Units 3.Serial/Version 4.LCD Contrast
Select "1.Printer" with the ter>.
key and confirm with 0.RS-232C 1.Printer 2.BarCode(AUX)
METTLER TOLEDO RE40D/RE50 Refractometers
21
Getting started
Select "GA-" for "Printer" with the with .
key and confirm
< Printer > Printer Exit
:IDP- DP:[Execute]
GA-
Other
6.2.1.3 Barcode reader Press the key. Select "0.Interface" with the <0> key and confirm with . Select "2.BarCode(AUX)" with the with .
key and confirm
< Interface > 0.RS-232C 1.Printer 2.BarCode(AUX)
Select "On" for "Barcode(AUX)", "9600" for "Baud Rate", "None" for "Parity", "1" for "Stop Bits" and "8" for "Data Bits" with the and keys. Confirm each setting with .
Enter "1" for "Start Pos." and "0" for "Read Length". Confirm both entries with . Select "CR+LF" for "Delimiter" with the key and confirm with .
< Barcode(AUX)> Barcode(AUX):Off On Baud Rate :<9600> Parity :Even Odd None Stop Bits :1 2 Data Bits :7 8 < Barcode(AUX)> Start Pos. Read Length Delimiter Exit
:[1] :[ 0] : :[Execute]
Press the key. The main display appears. To configure the barcode reader, scan in the two barcodes "Reset" and "Mode RS232" one after the other:
Reset
Mode RS232
To check whether the reader is functioning properly, scan in the barcode "Operator 1". If "Operator :" does not appear for a short time in the status line, check whether the barcode reader is connected properly and the settings in the "Barcode(AUX)" menu are correct.
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Operator 1
1.Method-1 Temp.(°C) Set 20.00 Cell 20.02
01-01 nD (None)
Operator : METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
6.2.2
User and country specific settings
6.2.2.1 Date and time Press the key. Select "1.Date & Time" and confirm with . Enter the date ("Day", "Month", "Year") and the time of day ("Hour", "Minutes"). Confirm your entries with . The date's format can be selected in the Setup menu under "5.International".
< Date & Time > 24/02/2002 15:18 Day :[24] Month :[ 2] Year :[2002]
Hour :[15] Minutes:[18] Exit :[Execute]
6.2.2.2 Operator names Press the key. Select "2.Op.Names/Units" and confirm with . Select "1.Operator Names" and confirm with .
< Op.Names/Units > 0.Concentration Units 1.Operator Names
Press the key to get to the input field "Name 1". Enter a list of future operators of the RE Refractometer (up to ten names may be entered) and confirm each name with . Press the key to enter capital/ small letters or numerals.
< Operator Names > Operator :<
>
Name 1 Name 2 Name 3
] ] ]
:[ :[ :[
If you have a barcode reader, make a photocopy of the list in appendix A.4.3 and fill in the names as you have entered them on the instrument.
6.2.3
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Activating the automatic error detection The "Repeat Meas." function enables the RE Refractometers to automatically detect the most frequent sources of errors in refractive index measurements. Please note that this function is only available if you use your RE Refractometer together with an automation unit (SC1 or SC30). Press the key. Select "7.Multiple Meas." (or "6.Multiple Meas.", RE40D) and confirm with . In the menu "Multiple Meas." select "2.Repeat Meas." and confirm with .
< Multiple Meas. > 0.Auto Start 1.Auto Statistics 2.Repeat Meas.
METTLER TOLEDO RE40D/RE50 Refractometers
23
Getting started
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Select "On" for "Repeat Meas." and confirm with . Further options appear in the "Repeat Meas." menu.
< Repeat Repeat Meas . Repetitions Movement Ratio SD Limit Exit
Enter 3 for "Repetitions" and 25 for "Movement Ratio". Enter a value of 0.00010 for "SD Limit" , if you work with an RE50 Refractometer. If you work with an RE40D Refractometer, enter a value of 0.0002 for "SD Limit". Confirm each entry with .
Meas. > :Off On :[3] :[ 25]% :[ 0.00010]nD :[Execute]
With the above settings, each sample will be measured three times: After the first measurement the sample is moved forwards twice in the system and measured again after each forward movement. If the standard deviation of the three measured refractive indices is above the value specified in "SD Limit" an error message is displayed and printed out. A detailed description of the "Repeat Meas." function can be found in section 12.8.3.
6.2.4
Setting up the instrument test
The measuring accuracy of the RE Refractometer needs to be checked from time to time with the built-in instrument test function (see section 11.6). In this section, the settings are shown for performing such instrument tests with distilled water. Press the key. Select "5.Set Check" (or "4.Set Check", RE40D) and confirm with . Set up the instrument test. Select "Daily" for "Check" < Set Check > with the key and confirm with . Enter the valCheck :Daily Periodic ues for "Ref.Value" (in our case the theoretical refractive Standard :[Water ] index of water at 20 °C, if you are working with an Ref.Value :[ 1.33299] Tolerance :[ 0.00005] RE40D enter a value of 1.3330) and for "Tolerance" Exit :[Execute] (the measured value's highest permissible deviation during the instrument test, if you are working with an RE40D enter a value of 0.0001) and the name of the standard ("Standard") according to the illustration on the right. Confirm each entry with .
6.2.5
Entering the method for adjustment
6.2.5.1 Deleting all methods Prior to entering the methods for adjustment and for the sugar determinations, you should delete all methods in the RE Refractometer's main memory (i.e., return them to the default settings): Press the key. Select "9.Memory Clear" (or "7.Memory Clear", RE40D) and confirm with . Select "4.Method Parameter" and confirm with .
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< Memory Clear > 0.Measured Data 1.Sample File 2.Periodic Check 3.Periodic Calib.
4.Method Parameter 5.All Parameter
METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
Select "Yes" for "Clear Execute" and confirm with . All of the RE Refractometer's methods are returned to the default settings.
< Method Parameter Clear > Clear Execute ? No Yes
6.2.5.2 Entering the parameters for adjustment Press the key. Select "0.CALIB." with the <0> key and confirm with . Method 0 is reserved for adjustment of the instrument. No measurements can be performed with this method!
Press the key. The "0.CALIB." method's parameters are displayed. The name of this method ("Method Name") and the temperature of the measuring cell ("Meas.Temp.") are displayed, but cannot be changed. The criterium for stability for acceptance of the measured value ("Stability") should always be set to 0 in method 0 (most accurate measurement), because this method is used for adjustment. The waiting time ("Wait Time") can also be left at 0 s.
No. Name 0.CALIB 1.Method-1 2.Method-2 3.Method-3 4.Method-4 Method 0
< Method List > Temp.(° C) 20.00 20.00 20.00 20.00
Result
nD nD nD nD
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[CALIB ] :[ 20.00]°C :[0] :[ 0]s :Off On
If you use your Refractometer without an attached automation unit, leave the setting for "Sequence" at "Off" and press the key.
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If your RE Refractometer is equipped with an automation unit, select "On" for "Sequence" with the key and confirm with . Additional lines for setting up the sequence appear in the menu. By setting up the sequence ("Sampling", "O.S.Rate", "Sampling Limit", "Drain", "Drain Rate", "Rinse-1", "Rinse-1 Time", "Rinse-2", "Rinse-2 Time", "Purge" and "Purge Time") you define the times for sampling as well as for draining, rinsing (with two different solvents) and drying of the measuring cell. Enter the settings for the sequence according to the illustrations on the right.
METTLER TOLEDO RE40D/RE50 Refractometers
Method 0
< Meas. Parameter >
Sampling O.S.Rate Sampling Limit Drain Drain Rate Method 0
:Off Set Auto :[ 120]% :[ 120]s :Off Set Auto :[ 100]%
< Meas. Parameter >
Rinse-1 Rinse-1 Time Rinse-2 Rinse-2 Time Purge
:Off :[ :Off :[ :Off
Set 15]s Set 10]s Set
25
Getting started
Confirm "Exit:[Execute]" with . i
6.2.6
A detailed description of the sequence settings can be found in section 9.5.
Method 0
< Meas. Parameter >
Purge Time Exit
:[ 240]s :[Execute]
Entering the method for measurements
A method for performing a measurement consists of three parts: the measuring parameters (access them with the key), the calculation parameters (entering of a calculation formula for the results, access the parameters with the key) and the settings for the printout of the results (access them with the key). On the whole, there are ten methods at your disposal, nine for your measurements and one for adjustment of the Refractometer (method 0). Please be aware that no measurements can be performed with method 0. Therefore, the , , , and the keys will not work when method 0 is selected as active method.
6.2.6.1 Entering the measurement parameters Press the key. Select method 1 ("Method-1") with the <1> key and confirm with .
No. Name 0.CALIB 1.Method-1 2.Method-2 3.Method-3 4.Method-4
< Method List > Temp.(° C) 20.00 20.00 20.00 20.00
Result
nD nD nD nD
Press the key. Enter "Fr.Juice" for "Method Name" and 0 for "Stability". Confirm both entries with . The measuring temperature ("Meas.Temp.") and the wait time ("Wait Time") can be left at their default settings.
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[Fr.Juice] :[ 20.00]°C :[0] :[ 0]s :Off On
If you use your Refractometer without an attached automation unit, leave the setting for "Sequence" at "Off" and press the key.
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METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
If your RE Refractometer is equipped with an automation unit, select "On" for "Sequence" with the and confirm with . Additional lines for setting up the sequence appear in the menu.
key
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By setting up the sequence ("Sampling", "O.S.Rate", "Sampling Limit", "Drain", "Drain Rate", "Rinse-1", "Rinse-1 Time", "Rinse-2", "Rinse-2 Time", "Purge" and "Purge Time") you define the times for sampling as well as for draining, rinsing (with two different solvents) and drying of the measuring cell. Enter the settings for the sequence according to the illustrations on the right. Confirm "Exit:[Execute]" with . A detailed description of the sequence settings can be found in section 9.5.
Method 1
< Meas. Parameter >
Sampling O.S.Rate Sampling Limit Drain Drain Rate Method 1
< Meas. Parameter >
Rinse-1 Rinse-1 Time Rinse-2 Rinse-2 Time Purge Method 1
:Off Set Auto :[ 150]% :[ 120]s :Off Set Auto :[ 100]%
:Off :[ :Off :[ :Off
Set 10]s Set 5]s Set
< Meas. Parameter >
Purge Time Exit
:[ 120]s :[Execute]
6.2.6.2 Entering the calculation parameters You will now define that the measuring results obtained with method 1 have to be displayed and printed out in BRIX (i.e., as sucrose content in percent by weight). Press the key. Select "0.Result" with the <0> key and confirm with . "2.Decimals" is to define the number of decimal places for the display and the printout of the results.
Method 1
Select "BRIX" for "Result" with the key and confirm with . Confirm "Exit:[Execute]" with .
Method 1
0.Result 1.Temperature Compensation 2.Decimals
Result Exit
METTLER TOLEDO RE40D/RE50 Refractometers
< Calc. Parameter >
< Result > : :[Execute]
27
Getting started
6.2.6.3 Setting the format for the printout of the results Press the key. The key allows you to determine the content of the printout of the results. Select 'GLP' for 'Format' with the key and confirm with . With this setting a complete list of all parameters is printed out after each measurement. A detailed description of the available formats for the printout of the results can be found in section 8.
6.3
Method 1
< Report >
Format Exit
: :[Execute]
Adjusting the RE Refractometer
According to the International Vocabulary of Basic and General Terms in Metrology from DIN, the operation of bringing a measuring instrument into a state of performance suitable for its use is called adjustment. The earlier used term "calibration" should not be used anymore when instrument settings are changed or adapted in order to ensure correct measurement values. Important: – The RE Refractometer must be turned on at least 30 minutes before it is adjusted. – To ensure correct measurements, the instrument must be adjusted at the measuring temperature. Adjust the RE Refractometer after each change of the measuring temperature. – Method 0 ("CALIB.") is reserved for adjusting the instrument, i.e., all the adjustments are done according to the settings of method 0 regardless of the currently selected method. Only the measuring temperature is adapted to the one of the currently selected method, because the instrument has to be adjusted at the same temperature as the samples are measured. This ensures that all the adjustments of the instrument are performed under the same conditions (i.e., the ones you defined in method 0). There is thus no need to select method 0 prior to adjustment of the instrument. – The results of the last 10 adjustments are stored in the instrument and may be displayed and printed out at any time (see section 11.7.2). With the barcode reader select your operator name from the list (see Appendix A.4.3). Your name appears in the status line of the display.
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
01-01 Brix(%)
Operator: Your name If you don't have a barcode reader, press the key, select "2.Op.Names/Units" and confirm with . Select "1.Operator Names" in the in the "Op.Names/Units" menu and confirm with . Select your name in the "Operator" field with the or key and confirm with . Press the key.
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METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
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Fill a sample vial to about 60% with distilled or deionized water or a water refractive index standard and seal it. Make sure that the slits in the cap's white membrane are facing downwards and that there are no air bubbles in the water!
Press the key and follow the instructions on the display: Open the cover lid and clean the measuring cell (the prism) thoroughly with water and ethanol. Wipe the prism dry with a soft paper tissue. Close cover the lid and press . The instrument is adjusted with air, the message "Calibrating" appears shortly on the display. Put distilled water or a water refractive index standard on the measuring cell until the ring mark is covered (approximately 0.4 mL). Close the cover lid and press . The message "Calibrating" flashes on the display during the adjustment to the water value. When the adjustment is done "OK" appears on the display and the result of the adjustment is printed out.
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
Clean Prism and Press Enter Key 1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
Set Water and Press Enter Key 1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
OK Calibration
If the instrument was not able to perform the adjustment, the error message "Failed" appears on the display instead of "OK". If this is the case, make sure that the water you used for adjustment is really of appropriate quality (i.e. distilled or correctly deionized). Clean the prism well, wipe it dry and repeat the adjustment. If the adjustment still does not succeed, contact your METTLER TOLEDO representative for technical assistance. Clean the measuring cell as described in section 5. Place the sample vial into the SC1 and confirm the message "Set Water and Press Enter Key" with the key on the RE Refractometer. The measuring cell is now cleaned and dried and then adjusted first with air and then with water. The message "Calibration OK" appears on the display and the result of the adjustment is printed out. At the end of the process the measuring cell is cleaned and dried again. i
The turntable of the SC30 rotates until position 1 is in front. On the display the message "Set Water at H.P. / Press Enter Key" appears. Place the sample vial in position 1 of the turntable and press the key on the RE Refractometer. The SC30's turntable rotates until the vial is at the sampling position. The measuring cell is now cleaned and dried and then adjusted first with air and then with water. The message "Calibration OK" appears on the display and the result of the adjustment is printed out. At the end of the process the measuring cell is cleaned and dried again.
METTLER TOLEDO RE40D/RE50 Refractometers
29
Getting started
If the instrument was not able to perform the adjustment (error message "Failed") please check the following and then repeat the adjustment: i
– Are the cleaning liquids connected properly, i.e., is the distilled water connected to the "Rinse 1" port and the highly volatile solvent (acetone) to the "Rinse 2" port? – Are all the tube connections tight? – Was the cap of the sample vial with the distilled water screwed tight and the white membrane properly in place? – Are all the settings for the sequence in method 0 ("CALIB.") correct (see section 6.2.5.2)?
6.4
Performing an instrument test and measurements
6.4.1
Performing instrument test and measurement manually or with SC1
6.4.1.1 Instrument test Select the operator name with the barcode reader or with the keypad as described in section 6.3. Press the key. The message "Set water and Press Enter Key" appears on the display.
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
Set water and Press Enter Key
Put distilled water or an water refractive index standard on the measuring cell until the ring mark is covered. Close the cover lid and press the key to start the instrument test. Fill a sample vial to about 60% with distilled or deionized water or a water refractive index standard, seal it and place it into the SC1. Press the key to start the instrument test. Confirm "Sampling Speed?" "Low" with . Confirm "Exit:[Execute]" with . The instrument test is performed. The result of the test is displayed and printed out.
If the instrument test fails, the error message "NG" appears on the display. If this is the case, repeat the instrument test. Should the instrument test fail a second time, the instrument needs to be readjusted (see section 6.3).
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
Ref.Value
nD
1.33299 -> 1.33298 OK Check(Daily) Ref.Value
nD
1.33299 -> 1.33200 NG Check(Daily)
Clean the measuring cell as described in section 5.
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METTLER TOLEDO RE40D/RE50 Refractometers
Getting started
6.4.1.2 Measurement Select the operator name with the barcode reader or with the keypad as described in section 6.3. Enter the name of your sample. If a barcode reader is available, scan in the barcode "Orange". The sample name ("Orange") appears in the status line of the display.
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
01-01 Brix(%)
Sample ID: Orange Orange If you don't have a barcode reader, press the key. A menu to enter the sample data (sample name and number) appears on the display. Enter "Orange" as "Sample ID" and confirm with . Press the key to toggle between capital/small letters and numerals. Confirm "Exit:[Execute]" with .
< Sample > Sample No. Sample ID Exit
:[01]-[01] :[Orange :[Execute]
]
Put orange juice on the measuring cell until the 1.Fr.Juice Orange 01-01 ring mark is covered. Stir the sample carefully Temp.(° C) Brix(%) in order to remove any air bubbles from the Set 20.00 Cell 20.00 surface of the prism. Close the cover lid and press the key. The measurement is started, during the measurement the message "Measuring" appears on the display. When the measurement has finished, the result is displayed and printed out. Clean the measuring cell as described in section 5.
11.28
Result
Fill a sample vial to about 80% with orange juice and seal it if you are not going to measure your sample immediately. Make sure that the slits in the cap's white membrane are facing downwards. Place the vial into the SC1. Press either the key on the RE Refractometer or the key on the SC1 to start the measurement. The measurement is started, during the measurement the message "Measuring" appears on the display. Please note that a triple determination of your sample is performed (automatic error detection, see section 6.2.3). When the measurements are done, the mean value of the three determinations is displayed and the mean value plus the standard deviation of the three results is printed out. Should the standard deviation of the three measured refractive indices be higher than the value you entered in the menu "Repeat.Meas" ("SD Limit", 0.00010 for the RE50, 0.0002 for the RE40D, respectively), the message "Out" appears on the display.
METTLER TOLEDO RE40D/RE50 Refractometers
1.Fr.Juice Temp.(° C) Set 20.00 Cell 20.00
Orange
Out Result
01-01 Brix(%)
11.28
31
Getting started
If this is the case, repeat the measurement. If the message "Out" appears again on the display your orange juice sample very probably contains a lot of solid particles (pulp) which cause scattered light and therefore measuring errors. If you need to do very accurate measurements (error < 0.1 BRIX) you have to filter the orange juice prior to measurement. If you can accept a lower accuracy for the results, you simply may enter a higher value for "SD Limit" in the "Repeat Meas." menu.
6.4.2
Performing instrument test and measurements with SC30
6.4.2.1 Preparing the samples, entering the sample data i
Prior to the measurements you will perform an instrument test. For this purpose, fill a sample vial to about 80% with distilled water and seal it. Fill another three sample vials to about 80% with your orange juice samples and seal them. Make sure that the slits in the white membrane (in the cap) are facing downwards. Place the sample vials in the SC30's turntable as follows (press the key on the SC30's keypad if required in order to rotate position 1 of the turntable in front): – Position 1: distilled water – Positions 2 … 4: orange juice Please make sure that method 1 is selected as the active method ("1.Fr.Juice" must appear on the upper left of the display). Press the key on the RE Refractometer in order to enter the sample data. The first line of this menu appears on the RE50 < Sample > Refractometer only (see section 13). Enter 4 Sample File :Skip Load Save for "No. of Samples" (instrument test + 3 No. of Samples :[ 4] samples of orange juice) and 1 for "Next Next Meas.No. :[ 1] Meas. No." (measurements are to begin with Method :Current Variable Parameters :Create Edit the first sample). Select "Current" for "Method" (the instrument test and all measurements are performed according to the same, i.e., the currently selected method) and "Create" for "Parameters" with the key and confirm with . Enter 2 for "No. of series" (2 series, instrument test and measurements) and confirm with . Confirm "Set Parameter:Execute" with in order to enter the sample data. Enter the sample data for the instrument test. With the barcode reader scan the barcode "CHECKSTD" (see following page) in the "Sample ID" field (sample identification). If you do not have a barcode reader, press the key when the cursor is in the "Sample ID" field and confirm with .
32
< Sample > No. of series Set Parameter Exit
< Sample >
:[2] :[Execute] :[Execute]
Series No.1(of 2)
Sample ID No.of samples High Sample No. Low Sample No. Method No.
:[CHECKSTD ] :[ 1] (1-1) :[ 1] :[ 1] :[1]
METTLER TOLEDO RE40D/RE50 Refractometers
Getting started i
Enter 1 for "No. of samples" (number of samples) and for the sample numbers ("High Sample No." and "Low Sample No.") and confirm your entries with . The "Method No." cannot be changed because you have selected "Current" for "Method" (see above). With this setting all measurements are performed with the same method (i.e., with the currently selected method). Select "Low" for "Sampling Speed" with the key and confirm with . Confirm "Next Series: [Execute]" with .
< Sample > Sampling Speed Next Series
Series No.1(of 2) :Low High :[Execute]
Enter the sample data for the orange juice < Sample > Series No.2(of 2) samples. With the barcode reader scan the Sample ID :[Orange ] barcode "Orange" (see below) in the "Sample No.of samples :[ 3] (2-4) ID" field (sample identification). If you do not High Sample No. :[ 2] Low Sample No. :[ 1] have a barcode reader, enter the sample name Method No. :[1] via the keypad and confirm with (press the key to enter capital/ small letters or numerals). Enter 3 for "No. of samples" (number of samples), 2 for "High Sample No.", and 1 for "Low Sample No.". Confirm your entries with . The "Method No." field may not be changed (see above). Select "Low" for "Sampling Speed" with the key and confirm with . Confirm "Save & Exit: [Execute]" with .
CHECKSTD
Sampling Speed Save & Exit Exit
Series No.2(of 2) :Low High :[Execute] :[Execute]
Orange
If you confirm "Edit" with , you can view a table of the data just entered (if you do not wish to do this, simply press the key.)
"Edit No." is the number of the sample to appear on the first line of the table. Confirm the default value 1 with . Confirm "Set Parameter" with and the table will appear.
METTLER TOLEDO RE40D/RE50 Refractometers
< Sample >
< Sample > Sample File No. of Samples Next Meas.No. Method Parameters
:Skip Load Save :[ 4] :[ 1] :Current Variable :Create Edit
< Sample > Edit No. Set Parameter Exit
:[ 1] :[Execute] :[Execute]
33
Getting started i
The table shows the running sample number ("No."), the measuring method ("M"), the two sample numbers ("S.No."), the sample identifications ("Sample ID") as well as the sampling speed ("Speed") for each sample.
No. 1 2 3 4
M 1 1 1 1
< Sample List> S.No. Sample ID 01-01 CHECKSTD 02-01 Orange 02-02 Orange 02-03 Orange
Speed Low Low Low Low
You can edit this table or enter the sample file directly in form of a table (see section 7.2.2).
6.4.2.2 Performing the instrument test and the measurements i
Select the operator name with the barcode reader or the keypad as described in section 6.3 and press the key. The instrument test and the measurements will be performed automatically in succession. The results are displayed after each measurement and printed out in GLP format. Please note that for each measurement (with the exception of the water for the instrument test) a triple determination is performed (automatic error detection, see section 6.2.3) and the means (and the standard deviations) of the three results are printed out. Should one of the standard deviations be higher than the value you specified, the message "Out" appears on the display and the error message "--- Out of limit ---" is printed out. If this error message appears for more than one sample, your orange juice sample probably contains a lot of solid particles (pulp) which cause scattered light and therefore measuring errors. If you need to do very accurate measurements (error < 0.1 BRIX) you have to filter your samples prior to measurement. If you can accept a lower accuracy for the results, you may simply enter a higher value for "SD Limit" in the "Repeat Meas." menu (see section 6.2.3). If the instrument test fails, a corresponding er1.Fr.Juice F 01-01 ror message ("NG", see illustration) appears Temp.(° C) Ref.Value nD on the display and the measurements of the Set 20.00 Cell 20.00 samples are not performed. If this is the case, please check whether the vials have been placed in the proper sequence on the turntable (i.e., that no orange juice sample was mistakenly used for the instrument test) and repeat the instrument test. Press the key on the SC30 until position 1 of the turntable is in front. Put in a new sample vial in position 1 of the turntable.
1.33299 -> 1.33200 NG Check(Daily)
Press the key. "Next Meas.No." < Sample > (number of the next measurement) now conSample File :Skip Load Save tains a 2 (because the instrument test has alNo. of Samples :[ 4] ready been performed). Overwrite this value Next Meas.No. :[ 1] Method :Current Variable with 1 and confirm with . Press the Parameters :Create Edit key. The instrument test is performed again and then the samples are measured. Should the instrument test fail a second time, the instrument needs to be readjusted (see section 6.3).
34
METTLER TOLEDO RE40D/RE50 Refractometers
Sample and sample file
7.
Sample (number/identification) and sample file
If a SC30 Sample Delivery and Cleaning Unit (sample changer) is attached to the RE Refractometer, the sample file always appears when you press the key. If no sample changer is connected (or if it has not been configured correctly, see section 6.2.1) and the sample file has been switched off (see section 11.2), a menu to enter data for a single sample appears.
7.1
Menu to enter data for a single sample If the sample file is switched off, when you press the key a menu to enter sample data (sample numbers and sample identification) appears.
< Sample > Sample No. Sample ID Exit
:[01]-[01] :[ ] :[Execute]
The sample number ("Sample No.") consists of two parts, e.g. [01]-[01]. The first two-digit number (ranging from 00 to 98) is the number of the measurement series. In the instrument it is referred to as the "High Sample No.". If you use your own specific series number for each type of sample when measuring various types of samples, it is easy to evaluate the stored results statistically afterwards (see section 11.1.1). The next two-digit number (ranging from 00 to 99) is automatically increased by 1 with each measurement. In addition to the two numbers, you can define a sample identification ("Sample ID", max. 10 characters, including space, dot, hyphen, etc.), e. g., a sample name or a batch number. The sample identification can be entered via the keypad or the barcode reader. If you are entering the sample identification with the keypad, you can toggle between capital and small letters and numerals with the key. To enter a sample identification with the barcode reader without changing the sample number, you do not have to press the key: Make sure that "Result", "Ready" or "Calibration" appears on the bottom line of the display and then scan the barcode. The sample identification will appear for a short time on the bottom line. If "Ready" was on the bottom line before entering the barcode, it will also appear in the first line,
1.Method-1 Temp.(° C) Set 20.00 Cell 20.00
01-01 nD(None)
Sample ID: water
If "Result" or "Calibration" was on the bottom line, the sample identification will only appear on the first line after the key has been pressed.
METTLER TOLEDO RE40D/RE50 Refractometers
35
Sample and sample file
7.2 i
Menu to enter a sample file (sample changer) If you operate your RE Refractometer together with a sample changer (SC30) or if the sample file has been switched on (see section 11.2), a menu to enter a sample file appears when you press the key: The first line ("Sample File") only appears on the RE50 Refractometer. This line is most often skipped, unless you wish to store a sample file onto a memory card or load a sample file from a memory card (see sections 13.1.8 and 13.1.10).
< Sample > Sample File No. of Samples Next Meas.No. Method Parameters
:Skip Load Save :[ 1] :[ 1] :Current Variable :Create Edit
"No. of Samples" is the number of samples to be measured. This number can be higher than 48 even though the turntable of the SC30 Sample Delivery and Cleaning Unit is only designed for 30 or 48 samples. "No. of Samples" can be changed during the measurement process. Example: Enter 12 for "No. of Samples" if you want to measure 12 samples. If an additional 13 samples are added after starting the measurement, you can increase the number to 25. "Next Meas No." is the number of the next measurement (according to the sample file). It is increased by 1 after each measurement. "Method" "Current" means that all measurements are performed with the same (i.e., currently selected) method. "Method" "Variable" allows measurements with various methods. Select "Parameters" "Create" and confirm with , if you want to enter the sample file in dialogue format. Select "Parameters" "Edit" when the sample file is to be displayed in the form of a table which can be edited. In the two following sections you can find a description of the input formats for sample files, either in dialogue format ("Create") or in table format ("Edit"), illustrated by the following example: Presuming you would like to: – measure a series of 12 grape juice and 7 orange juice samples. – perform an instrument test prior to the measurements (i.e., measure a water sample, see section 6.4.2.1). – measure the sample in two different ways: • by using different methods for each type of sample, i.e., method 1 for the instrument test (CheckStd), method 2 for the grape juice samples (GrapeJ.) and method 3 for the orange juice samples (OrangeJ.). • by using the same method (method 2, GrapeJ.) for the test and all measurements. First you must enter the three different methods: One for the instrument test (method 1, CheckStd), one for the grape juice (method 2, GrapeJ.) and one for the orange juice (method 3, OrangeJ.):
Method name Measuring temperature Stability
36
Method 1
Method 2
Method 3
CheckStd 20.00°C 0
GrapeJ. 20.00°C 1
OrangeJ. 20.00°C 2
METTLER TOLEDO RE40D/RE50 Refractometers
Sample and sample file
7.2.1 i
Creating a sample file using a dialogue format (Create) In this mode the sample file is created in a dialogue format. The RE Refractometer asks you how many series (group of samples) you want to measure (in our case three), which method is to be used for the measurements of each series, etc. If the sample's name cannot be entered with a barcode reader, or when the series is to be measured with different methods, then this is the quickest way of entering a sample file. In our example each type of sample is measured with a different method. Press the key. Enter 20 for "No. of Samples" (the whole series is made up of 20 samples: 1 test standard, 12 grape and 7 orange juice samples). Confirm your entry with . Move the cursor to "Method" and select "Variable" (with the key). Confirm with . Select or "Parameters" "Create" with the key and confirm with . Enter 3 for "No. of series" (number of series: test standard, grape and orange juice) and confirm with . Confirm "Set Parameter: [Execute]" with . While the cursor is in the "Sample ID" input field, press the key. "CHECKSTD" (instrument test) appears as sample identification. Confirm this with . Enter 1 for "No. of samples" (number of samples) and "Method No.", and confirm with . (For "High Sample No." and "Low Sample No." see section 7.1). You can leave the "Sampling Speed" at "Low". Move the cursor down and confirm "Next Series: [Execute]" with in order to enter the data for the second series (grape juice).
< Sample > Sample File No. of Samples Next Meas.No. Method Parameters
:Skip Load Save :[ 20] :[ 1] :Current Variable :Create Edit
< Sample > No. of series Set Parameter Exit
< Sample > Sample ID No.of samples High Sample No. Low Sample No. Method No.
< Sample > Sampling Speed Next Series
:[3] :[Execute] :[Execute]
Series No.1(of 3) :[CHECKSTD ] :[ 1] (1-1) :[ 1] :[ 1] :[1]
Series No.1(of 3) :Low High :[Execute]
If some of your samples are viscous you may set the sampling speed to "High" with the key so that those samples are pumped into the measuring cells at maximum speed (the sampling speed set on the SC30 then does not have any influence on the pumping speed).
METTLER TOLEDO RE40D/RE50 Refractometers
37
Sample and sample file i
Enter the sample identification (e.g., "GRAPE") with the keypad or the barcode reader (for a barcode example, see section 7.2.2). Confirm with . Enter 12 for "No. of Samples". Confirm with . Enter 2 for the "Method No." and confirm with . Move the cursor to "Next Series: [Execute]" and confirm with . Enter the sample identification (e.g., "ORANGE"), 7 for the "No. of samples" and 3 for the "Method No.". Confirm "Save & Exit:[Execute]" with .
< Sample > Sample ID No.of samples High Sample No. Low Sample No. Method No.
The sample file is displayed and you can print it out (with the key) or change it (see section 7.2.2). Press the key to leave the sample file. Now you can place the samples into the turntable of the SC30. Select the operator name (see section 12.3.2) and press the key to start the measurements.
38
Series No.3(of 3)
Sample ID No.of samples High Sample No. Low Sample No. Method No.
Sampling Speed Save & Exit Exit
Confirm the default value of 1 for "Edit No." (this is the sample that will appear on the first line of the table) with . Go to "Set Parameter:[Execute]" and confirm with .
:[GRAPE ] :[ 12] (2-13) :[ 2] :[ 2] :[2]
< Sample >
< Sample >
You can now look at the sample file you have created. To do this, confirm "Edit" with .
Series No.2(of 3)
:[ORANGE ] :[ 7] (14-20) :[ 1] :[14] :[3]
Series No.3(of 3) :Low High :[Execute] :[Execute]
< Sample > Sample File No. of Samples Next Meas.No. Method Parameters
:Skip Load Save :[ 20] :[ 1] :Current Variable :Create Edit
< Sample > Edit No. Set Parameter Exit
No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
M 1 2 2 2 2 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3
:[ 1] :[Execute] :[Execute]
< Sample List> S.No. Sample ID 01-01 CHECKSTD 01-02 GRAPE 01-03 GRAPE 01-04 GRAPE 01-05 GRAPE 01-06 GRAPE 01-07 GRAPE 01-08 GRAPE 01-09 GRAPE 01-10 GRAPE 01-11 GRAPE 01-12 GRAPE 01-13 GRAPE 01-14 ORANGE 01-15 ORANGE 01-16 ORANGE 01-17 ORANGE 01-18 ORANGE 01-19 ORANGE 01-20 ORANGE
Speed Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low
METTLER TOLEDO RE40D/RE50 Refractometers
Sample and sample file
7.2.2 i
Creating a sample file using a table format (Edit) In this mode, the sample file can be entered directly as a table. If all samples are to be measured with the same method and a barcode reader is used to enter the sample names, then this is the most efficient method to enter a sample file. In this section, you will find a description of how to enter a sample file with a barcode reader. Press the key, select method 1 ("GrapeJ.") and confirm with . Press the key. Enter 20 for the "No. of Samples" (the whole series consists of 20 samples) and confirm with . Move the cursor to "Method" and select "Current" (current method) with the key. Confirm with . Select "Edit" for "Parameters" and confirm with . Enter 1 for "Edit No." 1 and confirm with . Confirm "Set Parameter:[Execute]" with .
The sample file appears. Move the cursor to the first line of the column "Sample ID" and scan the barcode CHECKSTD:
CHECKSTD Then scan the barcode GRAPE twelve times
GRAPE and the barcode ORANGE seven times.
< Sample > Sample File No. of Samples Next Meas.No. Method Parameters
:Skip Load Save :[ 20] :[ 1] :Current Variable :Create Edit
< Sample > Edit No. Set Parameter Exit
No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
M 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
:[ 1] :[Execute] :[Execute]
< Sample List> S.No. Sample ID 01-01 01-02 01-03 01-04 01-05 01-06 01-07 01-08 01-09 01-10 01-11 01-12 01-13 01-14 01-15 01-16 01-17 01-18 01-19 01-20
Speed Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low Low
ORANGE The settings for the sampling speed ("Sp") can, if necessary (to measure viscous samples), be changed for each sample individually with the or key (confirm with ). Press the key to leave the sample file. Place the samples into the turntable of the SC30. Select the operator name (see section 12.3.2) and press the key to start the measurements.
METTLER TOLEDO RE40D/RE50 Refractometers
39
Report
8.
Report (password protected)
With the key you can define the content for the printout of the currently selected method's results. The report key is not active if method 0 ("CALIB.") has been selected. Select the method for which you wish to set the printout format ( key, see section 9) and then press the key. The following menu will appear: With the or key you can select between "Off", "Short", "GLP" and "Variable" for the printout's format. "Off" means no report is printed at the end of the measurements. "Short" only prints out the most important parameters (e.g., results, date and time, etc.) after each measurement. "GLP" provides a complete list of parameters after each measurement (see table below). If you chose "Variable" and confirm with , a list of parameters that can be printed out appears. You can choose the desired parameters individually by setting the parameter's option to "On" (the parameter is printed out) or "Off" (the parameter is not printed out) with the or key and confirming with .
Method 1
< Report >
Format Exit
Method 1
: :[Execute]
< Report >
Format Model/Serial Sample No. Date&Time Sample ID Method 1
< Report >
Method No. Meas.Temp. nD Temp.Comp. Result Method 1
: :Off On :Off On :Off On :Off On
:Off :Off :Off :Off :Off
On On On On On
< Report >
Meas.Time :Off On Operator Name:Off On Exit :[Execute]
Short Model, series, version Sample number Date and time Sample identification Method number and name Measuring temperature Refractive index Temperature compensation Results Duration of measurement Operator name
40
(Model/Serial) (Sample No.) (Date&Time) (Sample ID) (Method No.) (Meas.Temp.) (nD) (Temp.Comp.) (Result) (Meas.Time) (Operator Name)
X X
X X X
GLP X X X X X X X X X X X
Variable choice choice choice choice choice choice choice choice choice choice choice
METTLER TOLEDO RE40D/RE50 Refractometers
Measuring parameters
9.
Measuring parameters (password protected)
This section describes how measuring parameters can be defined for the methods. You have a total of 10 methods at your disposal. Method 0 is reserved for adjusting the instrument and is activated by pressing the key. Methods 1 to 9 are used for measurements. The default settings (preset values) for the parameters are as follows: Method 0: Parameter Method name Stability criteria Waiting time Sequence
Default setting (Method Name) (Stability) (Wait Time) (Sequence)
CALIB. 0 0s Off
The temperature of the measuring cell cannot be changed in method 0! When you press the key, it is carried over from the currently selected method! Methods 1 to 9: Parameter Method name Temperature measuring cell Stability criteria Waiting time Sequence
Default setting (Method Name) (Meas.Temp.) (Stability) (Wait Time) (Sequence)
Press the key. Select the method you would like to modify with the or key or enter the number of the method. Confirm your choice with .
METTLER TOLEDO RE40D/RE50 Refractometers
Method-x 20.00 °C 1 0s Off
No. Name 0.CALIB 1.Method-1 2.Method-2 3.Method-3 4.Method-4
< Method List > Temp.(° C) 20.00 20.00 20.00 20.00
Result nD nD nD nD
41
Measuring parameters
9.1
Method Name
Each method can be given a name (up to 8 characters). The name of method 0 ("CALIB") cannot be changed. Press the key. Press the key to delete the previous name ("Method Name"). Enter the desired name. Press the key to toggle between capital letters, small letters and numerals. Confirm your entry with .
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[Method-X] :[ 20.00]°C :[1] :[ 0]s :Off On
Note: Special characters can be entered with the barcode reader (see Appendix, section A.4.2).
9.2
Measuring temperature (Meas.Temp.)
Enter the desired measuring temperature ("Meas.Temp.", 15 to 50 °C for the RE50, 15 to 70 °C for the RE40D) and confirm with .
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[Method-X] :[ 20.00]°C :[1] :[ 0]s :Off On
Attention: – If the measuring temperature has been changed, the RE Refractometer must be readjusted. – After changing the measuring temperature you should give the instrument enough time (at least 30 minutes) to stabilize the temperature of the measuring cell before you adjust it.
9.3
Measurement stability (Stability)
This option allows you to speed up the measurements: You can select between high accuracy with longer measuring times and lower accuracy with shorter measuring times. Enter the desired measurement stability ("Stability", 0, 1 or 2) and confirm with . (0 = highest accuracy, longest measuring time).
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[Method-X] :[ 20.00]°C :[1] :[ 0]s :Off On
The repeatability of the measuring results not only depends on the value selected for "Stability", it also depends on the nature of the measured sample and the measuring conditions. You may roughly assume that the repeatability of the measuring results yielded with stability 0 is about 1 to 2 on the last digit of the resolution of the measuring instrument (nD, i.e. ± 0.00002 for the RE50 and ± 0.0001 for the RE40D ) and with stability 2 about 5 on the last digit.
42
METTLER TOLEDO RE40D/RE50 Refractometers
Measuring parameters
9.4
Waiting time (Wait Time)
The waiting time is the amount of time the instrument waits to start the measurement after the key has been pressed. The waiting time ensures that the sample has enough time to heat up or cool down to the measuring temperature. If the difference between sample and measuring temperature is more than 10 °C, you should implement a waiting time. Enter the desired waiting time ("Wait Time", 0 to 9999 s) and confirm with .
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
9.5
i
:[Method-X] :[ 20.00]°C :[1] :[ 0]s :Off On
Sequence (Sequence: sampling, draining, rinsing, purging) If you operate your RE Refractometer with an automation unit (SC1 or SC30), the sequence settings define the times for sampling as well as for draining, rinsing (with two different solvents) and drying of the measuring cell. Select "Sequence" "On" with the key to activate the sampling sequence. Confirm with .
Method 1
< Meas. Parameter >
Method Name Meas.Temp. Stability (0-2) Wait Time Sequence
:[Method-X] :[ 20.00]°C :[1] :[ 0]s :Off On
Select the type of sampling procedure ("Sampling"): Set: Enter the time for sampling in seconds. Auto: Recommended setting. The measuring cell detects the sample and turns off the pump automatically. Off: No sampling. If you have selected "Set", you must enter the sampling time ("Sampling Time", 0 to 9999 sec.). A sampling time of 10 to 15 seconds should suffice for most non-viscous samples (the sampling speed has to be set on the automation unit).
Method 1
If you have selected "Auto", you must enter an over-sampling rate ("O.S.Rate") with a time limit for sampling ("Sampling Limit").
Method 1
METTLER TOLEDO RE40D/RE50 Refractometers
< Meas. Parameter >
Sampling Sampling Time Drain Drain Rate Rinse-1
:Off Set Auto :[ 15]s :Off Set Auto :[ 100]% :Off Set
< Meas. Parameter >
Sampling O.S.Rate Sampling Limit Drain Drain Rate
:Off Set Auto :[ 150]% :[ 120]s :Off Set Auto :[ 100]% 43
Measuring parameters
i
With sampling set to "Auto", the RE Refractometer detects the markedly different measuring signal when the sample enters the measuring cell and turns the pump off according to the set over-sampling rate ("O.S.Rate", see below). The sampling time is, therefore, automatically adjusted to the viscosity of the sample. Attention: Please be aware that "Sampling Auto" only functions when the measuring cell is empty and more or less dry before sampling. If you want to use the automatic error detection ("Repeat Meas.", see section 11.8.3), then "Sampling" must be set to "Auto" in all methods. O.S.Rate:
The RE Refractometer measures the time the sample needs to get to the measuring cell after the pump has been activated and adds the "O.S. Rate" (over-sampling rate) to this time. Example: If the over-sampling rate has been set to 150% (recommended setting) and the sample needs 5 seconds to reach the measuring cell, then the pump stops after 12.5 seconds. The "O.S.Rate" ensures that impurities which might remain in the measuring cell (e.g., remaining rinsing liquid) are removed by the sample before the measurement is performed. In order to ensure accurate measurements you should thus (provided you have enough quantity of the samples to be measured) enter a rather high value for "O.S. Rate" (e.g., 200%).
Sampling Limit:
This is the maximum time for sampling. If no sample happens to be in the sample vial, the pump switches off automatically after this time has run out.
Select the type of procedure for draining the measuring cell ("Drain"): Set: Enter the time for draining in seconds. Auto: Recommended setting. The draining time is calculated based on the sampling time. Off: No draining.
Method 1
< Meas. Parameter >
Sampling O.S.Rate Sampling Limit Drain Drain Time
:Off Set Auto :[ 150]% :[ 120]s :Off Set Auto :[ 15]s
If you have selected "Set", you must enter the draining time ("Drain Time", 0 to 9999 sec.). A draining time of 15 to 25 seconds should suffice for most non-viscous samples. Setting the draining time of the measuring cell to "Auto" only makes sense if "Sampling" has also been set to "Auto" (recommended setting, see above).
Method 1
< Meas. Parameter >
Sampling O.S.Rate Sampling Limit Drain Drain Rate
:Off Set Auto :[ 150]% :[ 120]s :Off Set Auto :[ 100]%
The "Drain Rate" establishes how long draining shall take with respect to sampling. If the "Drain Rate" is set to 100% and the complete sampling procedure (including the over-sampling rate, see example above) takes 12.5 seconds, then the pump to drain the measuring cell will also be turned on for 12.5 seconds.
44
METTLER TOLEDO RE40D/RE50 Refractometers
Measuring parameters
i
The measuring cell can be rinsed with two solvents. First with a solvent ("Rinse-1") capable of dissolving the sample, and then with a highly volatile solvent ("Rinse-2") to ensure complete and quick drying of the measuring cell. Both rinsing cycles can be switched off ("Off") or on ("Set") individually. The time for the two rinsing procedures "Rinse-1 Time" (with solvent 1) and "Rinse-2 Time" (with solvent 2) is entered directly in seconds (0 to 9999 s).
Method 1
< Meas. Parameter >
Rinse-1 Rinse-1 Time Rinse-2 Rinse-2 Time Purge
:Off :[ :Off :[ :Off
Set 10]s Set 10]s Set
After rinsing, air is pumped through the measuring cell to dry it. Enter the drying time ("Purge"): Set: Enter the drying time in seconds ("Purge Time", 0 to 9999 s). Off: No drying of the measuring cell.
Method 1
< Meas. Parameter >
Rinse-1 Rinse-1 Time Rinse-2 Rinse-2 Time Purge Method 1
:Off :[ :Off :[ :Off
Set 10]s Set 10]s Set
< Meas. Parameter >
Purge Time Exit
:[ 120]s :[Execute]
Important: – If you want to work with "Sampling" "Auto", you must ensure that the time for drying ("Purge Time") is long enough to completely dry the measuring cell. – The sequence defined in method 0 ("Calib.") is tied to the key of the RE Refractometer. By pressing the key, the measuring cell is drained, rinsed and dried according to the sequence defined in method 0. – The sequence defined in method 0 is also carried out when the key is pressed, as long as the "Rinse / Purge" option in the "Changer" menu (see section 11.4) is set to "On", i.e., the measuring cell is cleaned before each adjustment according to the settings in the sequence of method 0. This guarantees that the measuring cell of the RE Refractometer is always clean and completely dry before an adjustment is performed. To ensure reliable adjustments of the RE Refractometer you should thus select the times for rinsing and drying of the measuring cell ("Rinse-1 Time", "Rinse-2 Time" and "Purge Time") in method 0 long enough to ensure a complete cleaning and drying of the measuring cell (see example in section 6.2.5.2). You should also select "On" for the parameter "Rinse Purge" in the "Changer" menu (see section 11.4).
METTLER TOLEDO RE40D/RE50 Refractometers
45
Calculation parameters
10.
Calculation parameters (password protected)
With the key you can define how the results of the currently selected method are to be calculated and displayed. The key is not active if method 0 ("CALIB.") has been selected. Select the method for which you want to set the calculation parameters ( key, see section 9) and then press the key.
10.1
Method 1
< Calc. Parameter >
0.Result 1.Temperature Compensation 2.Decimals
Result (refractive index, Brix, HFCS, concentration)
The RE Refractometers can display and print out the result of your measurements as refractive index (nD), as sugar content (BRIX, HFCS42, HFCS55, the latter two available on the RE50 only) and as a concentration calculated based on the measured refractive index. Press the key. Select "0.Result" and confirm with . Now you can select the desired unit for the result with the and keys. After confirming your choice for the unit of the result with , depending on the unit selected additional lines will appear in the "Result" menu's display.
Method 1 Result Exit
< Result > : :[Execute]
The following kinds of calculations are available for "Result": nD:
Refractive index, measured at the given temperature with the D-line of sodium (wavelength 589.3 nm).
BRIX:
BRIX is the term for the sucrose content of an aqueous sucrose solution in percent by weight (also called BRIX degrees). Conversion of the refractive index to BRIX is based on the table stored in the instrument (according to ICUMSA, see Appendix 2). This table contains only refractive index/BRIX data pairs valid at a temperature of 20 °C. If the measurements are performed at, for example, 40 °C, then the conversion of the refractive index into BRIX is done based on the ICUMSA table for 20 °C (thus, the results are not correct!). For this reason, if BRIX measurements are made at temperatures other than 20 °C, the temperature compensation must be activated (see section 10.3). With the temperature compensation activated, the RE Refractometer applies correction values according to OIML R108 (R124, resp.) in order to correct the BRIX values. Brix measurements of such samples as milk or soft drinks result in relative measurement values: the actual sucrose content is not determined, because the refractive index of such samples also depends on other contents (not only sucrose!) dissolved in the sample.
46
METTLER TOLEDO RE40D/RE50 Refractometers
Calculation parameters
HFCS:
(RE50 only). HFCS stands for High-Fructose Corn Syrup. These syrups are manufactured from natural corn syrup and consist of inverted (or isomerized) sugar, i.e., a mixture of dextrose, fructose, maltose and sucrose. They are classified according to their fructose content. Mainly three different HFCS are in use: a mixture containing 42% fructose (HFCS42), one containing 55% fructose (HFCS55) and a third one containing 90% fructose (HFCS90). Inverted sugar concentration denominates the concentration in weight % of an isomerized sugar solution. Inverted sugar concentration can be calculated from the refractive index of the inverted sugar solution measured at 20 °C (nD20). The RE50 Refractometer has built-in conversion tables ("Physical Properties Table", Corn Products, 1991) for two of the mixtures: HFCS42 and HFCS55. Since a temperature compensation table is also stored in this instrument, it is able to convert the measuring results for a temperature of 20 °C, as long as the measuring temperature is within the range of 20 to 50 °C and the temperature compensation is activated. See Appendix 3 for further information.
Conc.:
Determination of a concentration (normally in two component mixtures) based on the refractive index. The corresponding concentration tables (refractive indices / concentrations) with up to 30 data pairs per table can be entered for the calculations. These data pairs can be obtained either by measurement (i.e., the refractive indices of a series of solutions with a known concentration must be determined), by downloading them from our website www.refractometry.com or from the literature (e.g., "Handbook of Chemistry and Physics"). The concentrations are calculated based on first, second or third order polynomials. You can select the order of the polynomial, and the polynomial's coefficients are determined by means of a regression analysis by the RE Refractometer and then displayed. You can also enter the polynomial directly (i.e., without entering a concentration table). This allows the concentration function to be used to convert the refractive index into other units (e.g. Zeiss values).
User table:
(RE50 only). Similar to the above unit "Conc.", the User Tables are used to determine the concentration of two component mixtures. These tables are available on specific Memory Cards and can be downloaded directly into the RE50. Each table has a capacity of 200 data pairs (refractive index / concentration). Up to 9 tables consisting of 200 data pairs can be stored in the RE50 Refractometer. User Tables are only available on special request. Ask your local METTLER TOLEDO representative for further information.
METTLER TOLEDO RE40D/RE50 Refractometers
47
Calculation parameters
10.1.1 Calculating concentrations, converting into other units (Conc.) Select this type of calculation if you want to – determine the concentration of two-component mixtures based on the refractive index. – convert the refractive index into other units. Select "Conc." with the ter>.
key and confirm with
Result1 Conc.Unit Conc.Formula Parameter Set Data Replace
: : : :Table Coefficient :
First, you may define the unit (dimension) for your results. Select the desired unit ("Conc.Unit") with the and keys and confirm your choice with . The following units are available: none, %, ppm, mg/g, mg/mL, mg/L, g/L, mEq/L, mol/L as well as up to five freely definable names for units. These five names can be entered in the "Setup / Op.Names/Units / Concentration Units" menu (see section 12.3.1).
Method 1
< Result >
Result1 Conc.Unit Conc.Formula Parameter Set Data Replace
: : : :Table Coefficient :
There are two ways two to program a concentration formula: either you select a suitable formula (1/(A+BX) as well as polynomials of first, second or third order are available) and enter the corresponding coefficients directly, or you enter a concentration table (data pairs refractive index / concentration), select the desired formula. The RE Refractometer then determines the coefficients of the selected formula by regression analysis or it calculates the results by linear interpolation based on the table entered.
10.1.1.1 Direct entry of concentration formulas This section describes the procedure to enter a formula for converting the refractive index into another unit, the Zeiss number : 20
The formula to convert the refractive index (n D ) into Zeiss units (Zeiss, water = 15.00) is: 20
20
Zeiss = 2965.063 – 7007.752 • n D – 3596.889 • [n D ]2 The following steps have to be taken in order for the RE Refractometer to display the results of the refractive index measurements directly in Zeiss units: – Enter "Zeiss" as name for the results ("Setup"/"Op.Names/Units"/"Concentration Units" menu, see section 12.3.1). – Make sure that the measuring temperature ("Meas.Temp.") defined in the currently selected method is set to 20.00°C (see section 9.2). – Press the key. – In the "Calc.Parameter" menu, select "0.Result" and confirm with .
48
METTLER TOLEDO RE40D/RE50 Refractometers
Calculation parameters
– In the "Result" menu select "Conc." for "Result" with the key and confirm with (see section 10.1.1). – Select "Zeiss" for "Conc.Unit" with the confirm with .
key and
Method 1
< Result >
Result Conc.Unit Conc.Formula Parameter Set Data Replace
: : : :Table Coefficient ←nD :
– Select "A+Bx+Cx2" for "Conc.Formula" with the key and confirm with . – Select "Coefficient" for "Parameter Set" (direct entry of the concentration formula without a table) with the key and confirm with . – Select "x←nD" for "Data Replace" with the
key and confirm with .
– Enter the values for A, B and C according to the picture. Confirm each value with . – Confirm "Exit:[Execute]" with .
Method 1
< Result >
A B C Exit
:[ 2965.063]x10[ 0] :[-7007.752]x10[ 0] :[-3596.889]x10[ 0] :[Execute]
The RE Refractometer is now in a position to display the measured refractive index directly in Zeiss. The number of decimal places for the results can be defined under "Calc.Para/Decimals" (see section 10.3).
10.1.1.2 Entering concentration tables This section describes the procedure for entering a concentration table by means of an example: the determination of the glycerol content of an aqueous solution based on the refractive index. Concentration table for an aqueous glycerol solution (source: "Handbook of Chemistry and Physics"). Note: You can find further concentration tables on our website www.refractometry.com.
1 2 3 4 5 6 7 8 9 10
Concentration (in % by weight)
nD (at 20 °C)
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00
1.3330 1.3342 1.3353 1.3365 1.3376 1.3388 1.3400 1.3412 1.3424 1.3436
In order for the RE Refractometer to display and print out the measuring results directly in percent by weight of glycerol, the following steps must be taken: – Make sure that the measuring temperature ("Meas.Temp.") in the parameters of the currently selected method is set to 20.00°C (see section 9.2). – Press the key, select "0.Result" and confirm with .
METTLER TOLEDO RE40D/RE50 Refractometers
49
Calculation parameters
– Select "Conc." for "Result" with the key and confirm with (see section 10.1.1). – Select "%" for "Conc.Unit" with the firm with .
key and con-
– Select "A+Bx+Cx2" for "Conc.Formula" with the key and confirm with .
Method 1
< Result >
Result Conc.Unit Conc.Formula Parameter Set Data Replace
– Select "Table" for "Parameter Set" (entering a concentration table) with the (The parameter "Data Replace" may not be modified.)
: :<% > : :Table Coefficient ←nD-R :
key and confirm with .
– Enter 10 for "Data No." (number of data pairs) and confirm with .
Method 1
– Confirm "Enter Conc.Table:[Execute]" (entering a concentration table) with .
Data No.(3-30) :[10] Enter Conc. Table :[Execute] Exit :[Execute]
– Enter the data pairs according to the table. Confirm each value with .
Method No. 1 [ 2 [ 3 [ 4 [ Edit
1 < Conc.Table > Conc. nD 0.00000] [ 1.33300] 1.00000] [ 1.33420] 2.00000] [ 1.33530] 3.00000] [ 1.33650] Clear GetPara. Exit
Method No. 7 [ 8 [ 9 [ 10 [ Edit
1 < Conc.Table > Conc. nD 6.00000] [ 1.34000] 7.00000] [ 1.34120] 8.00000] [ 1.34240] 9.00000] [ 1.34360] Clear GetPara. Exit
– After all data pairs have been entered, select "GetPara." with the key and confirm with .
– The coefficients of the polynomial (A, B and C) as well as the graph of the curve (nD-R / concentration) are displayed. R is the mean of all refractive indices (and not the correlation coefficient!).
< Result >
< Get Parameter > [A+Bx+Cx2 ]Conc A: 4.531631x100 B: 8.506406x102 C:-2.777562x103 R: 1.338260
– Press . The concentrations are calculated using the coefficients. A table with the deviations between calculated and actual concentrations ("Error") is displayed.
X
Method 1 < Conc.Table > No. Error nD 7 [ 0.00342] [ 1.34000] 8 [ 0.00856] [ 1.34120] 9 [ 0.00569] [ 1.34240] 10 [-0.00507] [ 1.34360] Edit Clear GetPara. Exit
The values A, B and C are the coefficients of the selected function. R is the mean of all entered refractive indices. The RE Refractometer replaces the refractive indices for the regression analysis with the refractive indices minus the mean of all refractive indices (x←nD-R) in order to optimize the algorithm used (calculations with lower numbers). The values A, B, C and R can be used to enter the concentration function in a second RE Refractometer without having to enter the entire table. In this case, please be aware that "x←nD-R" must be selected for "Data Replace".
50
METTLER TOLEDO RE40D/RE50 Refractometers
Calculation parameters
– Press the key. The RE Refractometer can now display and print out the measured refractive indices directly as glycerol percent by weight in the range of 0 to 9% . The results' decimal places can be defined under "Calc.Para/Decimals" (see section 10.3).
10.2
Temperature compensation
Temperature compensation allows you to measure a sample at one temperature and to convert the measuring result to another temperature. Temperature compensation is utilized in the following cases: – The refractive index needs to be determined at e.g., 15 °C, but the sample is very viscous at that temperature. Such samples need to be heated in order to enable them to be pumped into the measuring cells. – To speed up the measurement. If, for example, the samples are at a temperature of 35 °C, but their refractive indices need to be determined at 15 °C, then you can set the cell temperature to 35 °C and convert the measured values to a temperature of 15 °C. – The refractive index needs to be determined at a temperature out of the RE Refractometer's range of measuring temperatures (e.g., at 100 °C). In this case, you can set the cell temperature to 50 °C and convert the measured values to a temperature of 100 °C. To use the temperature compensation, you need to know the temperature dependence of your sample's refractive index. There are two ways to enter the temperature dependence of the refractive index: – Entering a temperature compensation table (pairs of data made up of the temperature and the corresponding refractive index). In this case, the coefficient of the temperature compensation function is calculated by the RE50 Refractometer (this function is available only on this instrument). – Entering a coefficient for the temperature compensation. Hint If you have selected BRIX as unit for your measuring results and activated the temperature compensation, the results of your measurements are corrected if the measuring temperature is not 20.00 °C. This calculation is done based on a temperature compensation table (according to ICUMSA) stored in the instrument. – Press the key. Select "1.Temperature Compensation" and confirm with . – Select "Temp.Comp." "On" with the firm with .
key and con-
Method 1 Temp.Comp. Exit
METTLER TOLEDO RE40D/RE50 Refractometers
< Temp.Comp. > :Off On :[Execute]
51
Calculation parameters
10.2.1 Entering a temperature compensation table This function is available on the RE50 Refractometer only. The temperature dependency of the refractive index can be expressed as follows: nDc =
k • f(T)
The temperature dependency of the refractive index is contingent upon the composition of the sample and is therefore not equal for all samples. If only samples whose refractive indices have approximately the same temperature dependence are measured with one particular method, then you can determine the refractive index of this type of sample at various temperatures and enter the results (i.e., the data refractive index / temperature) into the RE50 Refractometer. The RE50 Refractometer then calculates the refractive index of the measured samples automatically for a particular temperature ("Comp.Temp"). The RE50 Refractometer performs these temperature compensation calculations based on polynomials of first, second or third order (the order of the polynomial can be selected) or by linear interpolation. These calculations are performed by the instrument as follows: f(Tc) To
n =
with •
D
n
TM
D
f(TM)
T
no
refr. index temperature compensated
Tc
reference temperature ("Comp.Temp.")
TM
measuring temperature
D
n
TM
refr. index at measuring temperature
D
f
polynomial function (determined by the RE50)
Enter the reference temperature ("Comp.Temp.") to Method 1 < Temp.Comp. > which the measurements need to be converted. ConTemp.Comp. :Off On firm it with . Select "Table" for "Parameter Set" Comp.Temp. :[ 20.00]°C with the key and confirm with . With the Parameter Set :Table Coefficient key, select the desired function ("Temp.Formula") for Temp.Formula : Data No. :[ 4] the temperature compensation: "Interpolation" (linear interpolation) or a polynomial of first, second or third order and confirm with . Enter the number of data pairs (refractive index / temperature) you want to enter ("Data No.") and confirm with . Confirm "Enter Temp.Table:[Execute]" with .
Method 1
< Temp.Comp. >
Enter Temp.Table Exit
Enter the temperature compensation table (data pairs refractive index / temperature). Confirm each entry with . Select "Get Para." with the key and confirm with .
52
:[Execute] :[Execute]
Method 1 < Temp.Table > No. Temp[°C] nD 1 [ 15.00] [ 1.46136] 2 [ 20.00] [ 1.45945] 3 [ 25.00] [ 1.45757] 4 [ 30.00] [ 1.45560] Edit Clear GetPara. Exit
METTLER TOLEDO RE40D/RE50 Refractometers
Calculation parameters
The coefficients (A, B, C and R, depending on the selected formula) and a graph of the curve (temperature / refractive index) are displayed. Please be aware that R is not a correlation coefficient. It is the mean of all entered temperatures.
< Get Parameter > [A+Bx+Cx2 ] nD A: 1.458514x100 B:-3.831940x10-4 C:-5.998332x10-7
By pressing the key again, the formula and the coefficients used to calculate the refractive indices for the different temperatures are displayed. The table displayed shows how well these calculated values coincide with the original data.
Method 1 < Temp.Table > No. Temp[°C] Error 1 [ 15.00] [-0.00001] 2 [ 20.00] [ 0.00002] 3 [ 25.00] [-0.00002] 4 [ 30.00] [ 0.00001] Edit Clear GetPara. Exit
R: 22.50000
10.2.2 Input of a coefficient for temperature compensation With this function only a linear temperature compensation is possible. For this reason you cannot enter a temperature compensation formula, but must enter a slope. Example: T
T
If the refractive index of a sample is 1.33340 (n 1) at 15°C (T1) and 1.33191 (n 2) at 30°C (T2) the "Slope" is D D calculated as follows: T
T
D
D
n1-n2 Slope • 1000 =
1.33340 - 1.33191 •
1000 =
T2 - T1
•
0.0993
30 - 15
Enter the reference temperature ("Comp.Temp."), to which the refractive indices need to be converted. Confirm with . With the key, select "Coefficient" for "Parameter Set" and confirm with (this parameter does not appear on the RE40D Refractometer). Calculate the "Slope" as described above and enter the value. Confirm with . Confirm "Exit:[Execute]" with .
METTLER TOLEDO RE40D/RE50 Refractometers
1000 =
Method 1
< Temp.Comp. >
Temp.Comp. Comp.Temp. Parameter Set Slope Exit
:Off On :[ 20.00]°C :Table Coefficient :[0.0993] / 1000 :[Execute]
53
Calculation parameters
10.3
Decimals
Press the key (see section 10). Select "2.Decimals" and confirm with . Enter the number of decimal places (i.e., places after the decimal point) for the display and printout of the results. Confirm each entry with .
Method 1
Confirm "Exit:[Execute]" with .
Method 1
nD nDt Brix Conc. HFCS42
HFCS55 Exit
nD: nDt: Conc.: Brix: HFCS42/55:
54
< Decimals > (0-5):[5] (0-5):[5] (0-2):[2] (0-5):[5] (0-2):[2] < Decimals > (0-2):[2] :[Execute]
Refractive index (RE40D: 0 to 4 decimal places) Temperature compensated refractive index (RE40D: 0 to 4 decimal places) Calculated concentrations (RE40D: 0 to 4 decimal places) Sucrose content in percent per weight (RE40D: 0 or 1 decimal place) Inverted sugar concentration (High-Fructose Corn Syrup) (available on the RE50 only)
METTLER TOLEDO RE40D/RE50 Refractometers
Functions
11.
Functions (password protected)
Press the key. If the password protection is RE40D Refractometer activated (see section 12.7) you will be prompted to < Function > enter the password. 0.Data File 4.Set Check Select the desired function by pressing the correspond1.Sample File 5.Periodic ing numeric key (keys <0> to <9>) or by using the 2.Changer 6.Multiple Meas. 3.DE Connect 7.Memory Clear arrow keys and confirm with . The "Function" menu is slightly different depending on the model of the RE Refractometer (see pictures). RE50 Refractometer The texts in braces (e.g., {"2.Changer"}) concern the < Function > RE40D Refractometer. Options which are not avail0.Data File 5.Set Check able on the RE40D Refractometer are written in gray 1.Sample File 6.Periodic letters (e.g., Load). 2.Method File 7.Multiple Meas. 3.Changer 4.DE Connect
8.CARD Utility 9.Memory Clear
11.1 Stored results (Function 0: Data File) The results of the last 100 measurements are automatically stored in the RE Refractometer. If 100 results have already been stored and a measurement is performed, then the oldest result is overwritten by the most recent (FIFO). The stored results can be accessed with the "Data File" function: you can do recalculations or statistical evaluations of the stored results or mark them as invalid so that they will not be included in statistical calculations. Furthermore, the RE50 Refractometer offers the possibility to save the stored results to a memory card or to reload them from a memory card into the instrument. Press the key. Select function "0.Data File" and confirm with